US5904996A - Method of manufacturing a magnetic field sensor - Google Patents

Method of manufacturing a magnetic field sensor Download PDF

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US5904996A
US5904996A US08/879,165 US87916597A US5904996A US 5904996 A US5904996 A US 5904996A US 87916597 A US87916597 A US 87916597A US 5904996 A US5904996 A US 5904996A
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exchange
layer
magnetic
biasing
sputter
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Pieter J. Van der Zaag
Hendrik T. Munsters
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Philips North America LLC
US Philips Corp
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US Philips Corp
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Assigned to PHILIPS ELECTRONICS NORTH AMERICA CORPORATION reassignment PHILIPS ELECTRONICS NORTH AMERICA CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: MUNSTERS, HENDRIK T., VAN DER ZAAG, PIETER J.
Assigned to U.S. PHILIPS CORPORATION reassignment U.S. PHILIPS CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: MUNSTERS, HENDRIK T., VAN DER ZAAG, PIETER J.
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
    • G01R33/00—Arrangements or instruments for measuring magnetic variables
    • G01R33/02—Measuring direction or magnitude of magnetic fields or magnetic flux
    • G01R33/06—Measuring direction or magnitude of magnetic fields or magnetic flux using galvano-magnetic devices
    • G01R33/09—Magnetoresistive devices
    • G01R33/093—Magnetoresistive devices using multilayer structures, e.g. giant magnetoresistance sensors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y25/00—Nanomagnetism, e.g. magnetoimpedance, anisotropic magnetoresistance, giant magnetoresistance or tunneling magnetoresistance
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S428/00—Stock material or miscellaneous articles
    • Y10S428/90—Magnetic feature
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/11—Magnetic recording head
    • Y10T428/1107—Magnetoresistive
    • Y10T428/1121—Multilayer

Definitions

  • an exchange-biasing layer comprising nickel oxide
  • magnetic heads which can be used to decrypt the magnetic flux emanating from a recording medium in the form of a magnetic tape, disc or card;
  • MRAMs Magnetic Random-Access Memories
  • nickel oxide as employed throughout this text should be interpreted as referring to any stoichiometric or non-stoichiometric compound of nickel and oxygen. Although the symbol “NiO” will frequently be used in this context, this symbol should be viewed as encompassing compounds of the form NiO 1 ⁇ , in which ⁇ is a positive fraction.
  • substrate should be interpreted as referring to any body of material on which the exchange-biasing layer can be provided; such a body may therefore be composite (e.g. in the case of a glass plate coated with a layer of another material). It should be explicitly noted that the magnetic layer may be located above or below the exchange-biasing layer.
  • exchange-biasing should be interpreted as encompassing both horizontal exchange-biasing (also referred to as longitudinal biasing) and vertical exchange-biasing (also referred to as perpendicular or transverse biasing).
  • a method as specified in the opening paragraph is known from European Patent Application EP 594 243, with the exception that the exchange-biasing layer therein described is comprised of an iron-manganese alloy (FeMn) instead of nickel oxide.
  • FeMn iron-manganese alloy
  • a first and a second layer of permalloy are magnetically coupled across an intervening layer of Cu, and the first permalloy layer is also exchange-biased with an adjacent FeMn layer.
  • the magnetization of the first permalloy layer is "pinned" in position; consequently, using an external magnetic field, the (free) magnetization of the second permalloy layer can be manipulated relative to the (fixed) magnetization of the first permalloy layer. Since the sensor's electrical resistance is dependent on the relative orientation of the magnetizations in the two permalloy layers, the sensor can thus be used to transcribe a fluctuating external magnetic flux into a correspondingly fluctuating electrical current.
  • FeMn is highly sensitive to oxidation and other corrosion, which can destroy its exchange-biasing properties, or at least cause them to radically deteriorate. This is particularly the case in so-called "sensor-in-gap" magnetic heads, which are used in hard disc memories.
  • oxidation barriers e.g. Ta layers
  • barriers tend to reduce the magnetic sensitivity of the sensor, and are seldom completely effective in the long term.
  • H eb is here defined as the field-axis displacement (from the zero-field line) of the hysteresis loop of an exchange-biased magnetic layer: see, for example, the article by R. Jungblut et al. in J. Appl. Phys. 75 (1994), pp 6659-6664.
  • the exchange-biasing layer is provided using sputter deposition in an Ar-gas atmosphere.
  • An advantage of sputter deposition is that it is highly compatible with large-scale, low-price industrial production, in contrast to techniques such as molecular beam epitaxy.
  • the inventors sputter-deposited a selection of NiO/permalloy bilayers on a glass substrate in an Ar atmosphere, using various Ar pressures, and subsequently measured the exchange-biasing field H eb for each NiO layer. It transpired that the value of H eb decreased with increasing Ar pressure.
  • the inventors interpreted this behaviour as an indication that lattice strain in the NiO, caused by Ar atoms at the substrate/NiO interface, was responsible to a significant extent for the exchange-biasing effects in the NiO, arguing that, at lower Ar pressures, more Ar atoms had the opportunity to settle into place at the said interface in the initiating NiO lattice.
  • the inventors have also observed that, in a sensor manufactured according to the invention, the magnetic coercivity H c of the magnetic layer is lower than when the employed sputter gas is Ar: see FIG. 5, for example.
  • a sensor advantageously has a larger dynamic range i.e. a larger range of external magnetic field strengths for which the magnetization in the magnetic layer remains "pinned" to the exchange-biasing layer.
  • a further advantage of the method according to the invention is that, when the exchange-biasing layer is deposited using Ne as a sputter gas (instead of Ar, for example), the exchange-biasing field H eb is less sensitive to (external) opposing demagnetizing fields.
  • This can, for example, be demonstrated by applying a (strong) oppositely oriented magnetic field to a field-cooled sensor structure, maintaining this reversing field for a prolonged time t (e.g. of the order of 100 hours), and using a Kerr magnetometer to measure hysteresis loops as a function of t (in rapid measurements lasting only about 10 seconds per loop). From such loops, H eb can be measured, and is found to vary much less (with t) in the case of a Ne-sputtered exchange-biasing layer than in the case of an Ar-sputtered exchange-biasing layer.
  • the invention does not require the sputter gas to be comprised entirely of Ne or He; for example, mixtures such as Ne+Ar or He+Ar also yield improved results with respect to pure Ar (see FIG. 4, for example).
  • the invention does not require the exchange-biasing layer to be comprised entirely of nickel oxide; for example, in a particular embodiment of the sensor according to the invention, the exchange-biasing layer may comprise a mixture of nickel oxide and cobalt oxide.
  • the material of the magnetic layer may, for example, comprise Fe, Ni, Co, or one of their alloys; in particular, permalloy is a suitable and widely-used choice.
  • AMR Anisotropic Magneto-Resistance
  • the magnetic layer is separated from a second magnetic layer by an interposed non-magnetic layer, so as to form a trilayer.
  • a non-magnetic layer may, for example, comprise Cu or Cr, and will typically have a thickness of the order of 1-5 nm.
  • the resulting sensor makes use of the so-called Giant Magneto-Resistance (GMR) effect, whereby the electrical resistance of the sensor depends on the relative orientation of the magnetizations in the two magnetic layers.
  • GMR Giant Magneto-Resistance
  • Another embodiment of the method according to the invention is characterized in that the sensor is provided with at least one flux guide, for the purpose of concentrating magnetic flux from an external source into the vicinity of the magnetic layer(s).
  • the sensor according to the invention may, if so desired, comprise various other layers besides those already referred to hereabove.
  • Such layers may, for example, include additional magnetic layers and non-magnetic layers (e.g. arranged in a spin-valve multilayer structure), additional exchange-biasing layers, adhesion promoting layers (e.g. comprising Ta), anti-oxidation layers (e.g. comprising SiO 2 or Si 3 N 4 ) or wear-resistant layers (e.g. comprising Cr 2 O 3 ).
  • the quantity of Ne or He typically incorporated at the substrate/NiO interface is in excess of 10 12 atoms/cm 2 , and generally of the order of about 10 13 atoms/cm 2 .
  • the presence of such Ne or He can be (quantitatively) verified using such analysis techniques as Thermal Gas Desorption (see, for example, FIG. 6). Since, as already set forth hereabove, the advantages associated with the inventive method are believed to derive (at least to a substantial extent) from the presence of Ne and/or He atoms at the substrate/NiO interface, the inventors also lay claim to a sensor as specified in claims 4 and 5.
  • such a sensor may, for example, be manufactured using Ne-ion implantation and/or He-ion implantation together with vapour deposition or laser ablation deposition; alternatively, such deposition may be performed in a partial Ne and/or He atmosphere.
  • FIG. 1 is a perspective view of part of a particular embodiment of a magnetic field sensor (AMR sensor) according to the invention
  • FIG. 2 is a cross-sectional view of part of an alternative embodiment of a magnetic field sensor (GMR sensor) according to the invention
  • FIG. 3 renders a perspective view of a magnetic read head (magnetic field sensor) according to the invention, having flux guides and electrical connections;
  • FIG. 4 graphically depicts the dependence of the exchange-biasing field H eb (kA/m) on the sputter-gas pressure p s (Pa) for sputter-deposited glass/NiO/permalloy samples, using various sputter gases;
  • FIG. 5 graphically depicts the dependence of the coercive field H c (kA/m) on the sputter-gas pressure p s (Pa) for the same samples to which FIG. 4 pertains;
  • FIG. 6 graphically depicts the results of Thermal Gas Desorption experiments conducted upon magnetic field sensors according to the invention, revealing the presence of Ne atoms in such sensors.
  • FIG. 1 renders a perspective view of part of a magnetic field sensor according to the invention.
  • a sensor can be manufactured as follows.
  • a non-magnetic substrate 1 e.g. Si
  • a uniform layer of soft magnetic material e.g. a CoZrNb alloy.
  • this layer is subsequently formed into two strips 10 which face each other across an intervening gap 12; in this manner, two flux guides 10 are created on the substrate 1.
  • the substrate 1 is provided with two "blocks" 2 of NiO, which straddle the flux guides 10.
  • the NiO is sputter-deposited in a HV magnetron device using Ne as a sputter gas, and employing, for example, the following sputter parameters:
  • substrate-holder temperature 200° C.
  • the area between the blocks 2 is subsequently filled with a body 11 of electrically insulating material (e.g. SiO 2 ), flush with the upper surface of the blocks 2.
  • a strip-like "bridge" 3 of magneto-resistive material e.g. permalloy is then provided on top of the blocks 3 and across the body 11.
  • the device thus created therefore has a layered structure which consecutively comprises a substrate 1, an exchange-biasing layer 2, and a magnetic layer 3 which is exchange-biased to the layer 2 and which acts as an AMR sensor.
  • a layered structure which consecutively comprises a substrate 1, an exchange-biasing layer 2, and a magnetic layer 3 which is exchange-biased to the layer 2 and which acts as an AMR sensor.
  • the device further comprises flux guides 10 and an intervening gap 12 which are so arranged that concentrated magnetic flux carried by the guides 10 emerges from the gap 12 and intercepts the magnetic layer 3.
  • FIG. 2 cross-sectionally depicts part of a particular embodiment of a magnetic field sensor according to the invention.
  • This sensor has a stacked structure which consecutively comprises a substrate 1, an exchange-biasing layer 2 which comprises NiO, a first magnetic layer 3 which is exchange-biased with the layer 2, a non-magnetic layer 4 and a second magnetic layer 5.
  • the layers 3,4,5 form a spin-valve trilayer.
  • the layer 2 has been provided by HV magnetron sputter-deposition, using Ne as a sputter gas.
  • the particular sputter parameters in this case were as follows:
  • substrate-holder temperature 200° C.
  • the substrate 1 comprises a glass plate.
  • the magnetic layers 3,5 may, for example, comprise Fe, Co, Ni, or one of their alloys (such as permalloy).
  • the non-magnetic layer 4 may, for example, comprise Cu. Exemplary thicknesses for the various layers are as follows:
  • the magnetic layers 3,5 are ferromagnetically coupled to one another across the intervening layer 4. Consequently, in the absence of an external magnetic field, the magnetizations in the layers 3,5 will be mutually parallel.
  • so-called magnetic annealing is employed during growth of the magnetic layers 3,5 so as to achieve a situation whereby their magnetizations are substantially mutually perpendicular in the absence of an external magnetic field.
  • a sensor is, for example, elucidated in EP 594 243 (in which, however, the employed exchange-biasing material is FeMn instead of NiO).
  • FIG. 3 renders a schematic perspective view of part of a magnetoresistive magnetic read head (magnetic field sensor) according to the invention.
  • the head comprises a transducer S (e.g. an AMR sensor as described in Embodiment 1 or a GMR sensor as described in Embodiment 2) with electrical connections 65.
  • the head additionally comprises flux guides 59,59', which are positioned relative to the transducer S so as to form a magnetic circuit.
  • the end faces 61,61' form part of the pole face of the head, the magnetic gap 63 being located between said faces 61,61'.
  • the head may also contain an electrical coil, which can be employed in the recording of magnetic information on magnetic media.
  • FIG. 4 graphically depicts the dependence of the exchange-biasing field H eb (in kA/m) on sputter-gas pressure p s (in Pa) for sputter-deposited glass/NiO/permalloy samples, using various sputter gases (Ar, Ar+Ne, Ar+He, Ne). All of the sputtered samples had the following composition:
  • the lines in the graphs serve as guides to the eye.
  • FIG. 5 graphically depicts the dependence of the coercive field H c (in kA/m) on sputter-gas pressure p s (in Pa) for the same glass/NiO/permalloy samples referred to hereabove. It is evident from the graph that, for any given value of p s , the corresponding value of H c is highest for Ar, and considerably lower when the employed sputter gas comprises Ne or He.
  • FIG. 6 graphically depicts the results of Thermal Gas Desorption experiments conducted upon magnetic field sensors according to the invention, revealing the presence of Ne atoms in such sensors.
  • a field sensor such as that elucidated in Embodiment 1 was placed in a vacuum chamber fitted with a Zr--C getter.
  • Each sample was placed in a quartz tube, and was heated to a temperature of approximately 500° C., after evacuation of the chamber to a given background pressure. This temperature was maintained for a prolonged time t, causing the escape of Ne gas from the samples, together with "unwanted" gases such as H 2 O, CO 2 , C x H y , etc.
  • the getter was maintained at a temperature of about 400° C., and absorbed these unwanted gas atoms; the Ne, however, was not absorbed by the getter, allowing the quantity Q Ne of escaped Ne atoms to be determined using mass spectrometry.
  • FIG. 6 renders a plot of Q Ne (Pa.1/m 2 ) as a function of t (hours) for various sensors, each having being manufactured using a different Ne sputter-gas pressure during provision of the exchange-biasing layer (viz. 6 mTorr ( ⁇ ), 8 mTorr ( ⁇ ) and 11 mTorr ( ⁇ )).
  • the graph clearly reveals the presence of Ne atoms in all the sensors.
  • the NiO exchange-biasing layer is in contact with the substrate.
  • the inventors manufactured several "inverted" sensor structures having the following composition:
  • the Ni 80 Fe 20 layer was sputtered in Ar at a pressure of 5 mTorr and in a magnetic field of 15 kA/m.
  • the NiO exchange-biasing layers in the various sensors were sputtered using different sputter gases and at various sputter-gas pressures, as listed in the following table.
  • the (sputter) gas pressure is expressed in mTorr.
  • H eb and H c are expressed in Oe, and were determined using a SQUID magnetometer (at 290 K). All depositions occurred at room temperature.

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Hall/Mr Elements (AREA)
  • Measuring Magnetic Variables (AREA)
  • Thin Magnetic Films (AREA)
US08/879,165 1996-07-05 1997-06-19 Method of manufacturing a magnetic field sensor Expired - Fee Related US5904996A (en)

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EP96201884 1996-07-05
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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6184680B1 (en) * 1997-03-28 2001-02-06 Tdk Corporation Magnetic field sensor with components formed on a flexible substrate
US6266217B1 (en) * 1996-01-31 2001-07-24 U.S. Philips Corporation Magnetic head having an anti-ferromagnetic oxide layer between a flux guide and a magneto-resistive sensor
US6275033B1 (en) * 1997-07-01 2001-08-14 U.S. Philips Corporation Magnetic field sensor having nickel oxide and cobalt containing ferromagnetic layers
US6306311B1 (en) 1999-11-01 2001-10-23 Headway Technologies, Inc. Method to make a high data rate stitched writer for a giant magneto-resistive head
WO2001094963A3 (de) * 2000-06-09 2002-04-04 Inst Physikalische Hochtech Ev Wheatstonebrücke, beinhaltend brückenelemente, bestehend aus einem spin-valve-system, sowie ein verfahren zu deren herstellung
US6650112B2 (en) * 1998-08-05 2003-11-18 Minebea Co., Ltd. Magnetics impedance element having a thin film magnetics core
US20040239321A1 (en) * 2003-06-02 2004-12-02 The Foundation: The Research Institute For Electric And Magnetic Materials Thin film magnetic sensor and method of manufacturing the same
US20040239320A1 (en) * 2003-05-28 2004-12-02 The Foundation: The Research Institute For Electric And Magnetic Materials Thin film magnetic sensor and method of manufacturing the same
US20040246649A1 (en) * 2003-06-03 2004-12-09 Mks Instruments, Inc. Flow control valve with magnetic field sensor
US20060084198A1 (en) * 2002-09-27 2006-04-20 Thales Electrostatically actuated low response time power commutation micro-switches
US10816615B2 (en) * 2017-05-19 2020-10-27 Asahi Kasei Microdevices Corporation Magnetic sensor

Citations (2)

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EP0594243A2 (en) * 1992-10-19 1994-04-27 Koninklijke Philips Electronics N.V. Magnetic field sensor
JPH08129721A (ja) * 1994-09-08 1996-05-21 Sumitomo Metal Ind Ltd ＮｉＯ反強磁性膜の製造方法並びに磁気抵抗効果素子の製造方法とその素子

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US5446613A (en) * 1994-02-28 1995-08-29 Read-Rite Corporation Magnetic head assembly with MR sensor
JP2738312B2 (ja) * 1994-09-08 1998-04-08 日本電気株式会社 磁気抵抗効果膜およびその製造方法
JP2748876B2 (ja) * 1995-01-27 1998-05-13 日本電気株式会社 磁気抵抗効果膜
JPH0983039A (ja) * 1995-09-14 1997-03-28 Nec Corp 磁気抵抗効果素子

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EP0594243A2 (en) * 1992-10-19 1994-04-27 Koninklijke Philips Electronics N.V. Magnetic field sensor
JPH08129721A (ja) * 1994-09-08 1996-05-21 Sumitomo Metal Ind Ltd ＮｉＯ反強磁性膜の製造方法並びに磁気抵抗効果素子の製造方法とその素子

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Exchange anisotropy in coupled films of Ni81 Fe19 with NiO and Cox NI1-x O. M.J. Carey and A.E. Berkowitz. American Institute of Physics, vol. 60, No. 24, Jun. 15, 1992, pp. 3060-3062.
Exchange coupling between NiO and NiFe thin films. J.X. Shen and M.T. Kief. American Institute of Physics, vol. 79, No. 8, Apr. 15, 1996, pp. 5008 5010. *
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Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6266217B1 (en) * 1996-01-31 2001-07-24 U.S. Philips Corporation Magnetic head having an anti-ferromagnetic oxide layer between a flux guide and a magneto-resistive sensor
US6184680B1 (en) * 1997-03-28 2001-02-06 Tdk Corporation Magnetic field sensor with components formed on a flexible substrate
US6275033B1 (en) * 1997-07-01 2001-08-14 U.S. Philips Corporation Magnetic field sensor having nickel oxide and cobalt containing ferromagnetic layers
US6650112B2 (en) * 1998-08-05 2003-11-18 Minebea Co., Ltd. Magnetics impedance element having a thin film magnetics core
US6306311B1 (en) 1999-11-01 2001-10-23 Headway Technologies, Inc. Method to make a high data rate stitched writer for a giant magneto-resistive head
US6583966B2 (en) 1999-11-01 2003-06-24 Headway Technologies, Inc. Method to make a high data rate stitched writer for a giant magneto-resistive head
US6882145B2 (en) 2000-06-09 2005-04-19 Institut Fuer Physikalische Hochtechnologie E.V. Wheatstone bridge containing bridge elements, consisting of a spin-valve system and a method for producing the same
WO2001094963A3 (de) * 2000-06-09 2002-04-04 Inst Physikalische Hochtech Ev Wheatstonebrücke, beinhaltend brückenelemente, bestehend aus einem spin-valve-system, sowie ein verfahren zu deren herstellung
US20040023064A1 (en) * 2000-06-09 2004-02-05 Arno Ehresmann Wheatstone bridge containing bridge elements, consisting of a spin-valve system and a method for producing the same
US20060084198A1 (en) * 2002-09-27 2006-04-20 Thales Electrostatically actuated low response time power commutation micro-switches
US7297571B2 (en) * 2002-09-27 2007-11-20 Thales Electrostatically actuated low response time power commutation micro-switches
US20040239320A1 (en) * 2003-05-28 2004-12-02 The Foundation: The Research Institute For Electric And Magnetic Materials Thin film magnetic sensor and method of manufacturing the same
US20040239321A1 (en) * 2003-06-02 2004-12-02 The Foundation: The Research Institute For Electric And Magnetic Materials Thin film magnetic sensor and method of manufacturing the same
US20060226835A1 (en) * 2003-06-02 2006-10-12 The Foundation: The Research Institute For Electric And Magnetic Materials Methods for manufacturing a thin film magnetic sensor
US7170287B2 (en) * 2003-06-02 2007-01-30 The Foundation : The Research Institute For Electric And Magnetic Materials Thin film magnetic sensor and method of manufacturing the same
US7218103B2 (en) 2003-06-02 2007-05-15 The Foundation: The Research Institute For Electric And Magnetic Materials Methods for manufacturing a thin film magnetic sensor
US20040246649A1 (en) * 2003-06-03 2004-12-09 Mks Instruments, Inc. Flow control valve with magnetic field sensor
US10816615B2 (en) * 2017-05-19 2020-10-27 Asahi Kasei Microdevices Corporation Magnetic sensor

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WO1998001762A2 (en) 1998-01-15
EP0910800A2 (en) 1999-04-28
EP0910800B1 (en) 2004-02-11
JP2000500292A (ja) 2000-01-11
DE69727574T2 (de) 2004-12-16
DE69727574D1 (de) 2004-03-18
WO1998001762A3 (en) 1999-04-15

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